NOAA NST: 160.0: Trace metals in marine sediments by X-ray fluorescence

Summary
Analytes
Revision
Data and Sites

Official Method Name

X-Ray fluorescence for the analysis of trace metals in marine sediments.

Current Revision

March 1998

Media

SOILS/SEDIMENT

Instrumentation

X-Ray Fluoresence

Method Subcategory

Inorganic

Method Source

NOAA NST

Citation

Sampling and Analytical Methods of the National Status and Trends Program Mussel Watch Project: 1993-1996 Update.
NOAA Technical Memorandum NOS ORCA 130. March 1998. Silver Spring, MD. 233pp.

Brief Method Summary

Sample preparation and analysis methods have been developed and refined that allow accurate and precise determination of major and trace elements in sediment samples. Sample preparation emphasizes homogenization and total digestion steps that minimize contamination. Analysis includes a full suite of quality assurance samples (emphasis on certified reference materials) in order to produce reliable data. These methods allow measurement of both background and elevated concentrations within NOAA's Status and Trends Program, permitting subtle temporal and spatial differences to be detected.

Scope and Application

This method measures trace metals (at ug / g concentrations) in marine sediments.

Applicable Concentration Range

0.1-1000.0

Interferences

Spectral interferences may be minimized by sample dilution, use of an alternate analyte wavelength, or selective volatilization of the analyte. Non-spectral interferences may be detected and compensated for using the method of standard additions.

Quality Control Requirements

The quality assurance / quality control requirements are initial calibration and continuing calibration checks, method blank analysis, surrogate compound analysis, matrix spike analysis, and reference sample analysis.

Sample Handling

Sediments are obtained with a grab sampler that collects the top 2 cm of surface sediment. Sample aliquots are weighed, freeze-dried for approximately 5 days to constant weight in 125-mL polystyrene Spex jars in a freeze dryer, and reweighed to determine percent dry weight. Approximately 3 g are ground for 5 min using a Spex ceramic ball mill.

Maximum Holding Time

6 months (frozen)

Relative Cost

$201 to $400

Sample Preparation Methods

NOAA TM #130

This method has 9 analytes associated with it.

Analyte	Detection Level	Bias	Precision
Aluminum(7429-90-5) Al Aluminium Aluminum Aluminum (fume or dust) Aluminum powder	100.000 ug/g	N/A	0.40 RSD
Arsenic(7440-38-2) Arsenic As	0.100 ug/g	N/A	0.30 RSD
Chromium(7440-47-3) Chromium Cr	0.050 ug/g	N/A	0.50 RSD
Copper(7440-50-8) Copper Copper (metallic) Cu	0.400 ug/g	N/A	0.40 RSD
Iron(7439-89-6) Fe Iron	11.000 ug/g	N/A	0.20 RSD
Lead(7439-92-1) Lead Lead and compounds (inorganic) Lead and lead compounds Pb	0.200 ug/g	N/A	0.50 RSD
Manganese(7439-96-5) Manganese Mn	2.500 ug/g	N/A	0.40 RSD
Nickel(7440-02-0) Ni Nickel Nickel, soluble salts Raney Nickel (R)	0.300 ug/g	N/A	0.70 RSD
Zinc(7440-66-6) Zinc Zinc (fume or dust) Zinc and Compounds Zn	0.800 ug/g	N/A	0.10 RSD

Precision Descriptor Notes:	Precision and accuracy data were obtained from NOAA's NS&T interlaboratory validation QA program. NOAA Technical memorandum NOS ORCA 142 "National Status and Trends Program Thirteenth Round Intercomparison Exercise Results for Trace Metals in Marine Sediments and Biological Tissues".
Detection Level Note:	Federal Register (1984), Vol. 49, No. 209: 198-199.

Revision	PDF/Link
March 1998

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NOAA NST: 160.0: Trace metals in marine sediments by X-ray fluorescence

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